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建立了猪肉中万古霉素、去甲万古霉素和杆菌肽A 3种多肽类抗生素的正压驱动固相萃取法结合超高效液相色谱串联三重四极杆质谱(UHPLC-MS/MS)检测方法。猪肉样品经提取后正己烷脱脂,采用Pharma FF C_(18)固相萃取小柱正压驱动净化,洗脱液无需浓缩直接进行LCM S/M S分析,使用0.1%甲酸水溶液和乙腈分别作为流动相进行梯度洗脱,采用溶剂共进样方式分析,ESI正离子模式,前体离子均为双电荷离子,多反应监测(MRM)模式检测,外标法定量。结果表明,3种多肽抗生素采用基质加标曲线定量,在0.5~100μg/L范围内线性关系良好,相关系数均大于0.999,方法定量限为0.40~0.70μg/kg;加标回收率在72.9%~82.0%之间,相对标准偏差(RSD)为2.6%~14%。方法适用于猪肉中3种多肽类抗生素的同时测定。
A pressure-driven solid-phase extraction coupled with ultra-performance liquid chromatography tandem triple-quadrupole mass spectrometry (UHPLC-MS / MS) was developed to detect vancomycin, norvancomycin and bacitracin A in pork. method. The samples of pork were degreased with n-hexane and purified with a positive pressure of Pharma FF C_ (18) solid-phase extraction cartridges. The eluate was directly analyzed by LCM S / MS without concentration using 0.1% formic acid in water and acetonitrile as the mobile phase Gradient elution was carried out by solvent co-injection method. ESI positive ion mode and precursor ions were double-charged ions. Multiple reaction monitoring (MRM) mode detection and external standard method were used for quantification. The results showed that the three kinds of polypeptide antibiotics were quantified by matrix spike curve, and the linearity was good in the range of 0.5-100 μg / L with the correlation coefficients greater than 0.999. The limit of quantification was 0.40-0.70 μg / kg. The spiked recoveries were 72.9% ~ 82.0%, the relative standard deviation (RSD) was 2.6% ~ 14%. The method is suitable for the simultaneous determination of three polypeptide antibiotics in pork.